水复合溶剂体系茴脑臭氧化反应合成茴香醛新工艺

New Process for Preparation of Anisaldehyde Based on Ozonolysis of Anethole in Mixture Solvent System

以茴脑为原料,有机溶剂与水复合溶剂为溶剂,室温下通过臭氧化分解反应制取茴香醛,并通过GC-MS、FT-IR和1H-NMR对产品进行了表征。对该溶剂体系与传统溶剂体系下茴香醛的产率进行了对比,并确定了丙酮/水体系为最佳溶剂体系。实验详细考察了溶剂用量、臭氧气流量、混合溶剂中水含量和反应时间等工艺参数。优化的工艺条件为:丙酮和水为溶剂,m(茴脑):m(混合溶剂)=1:3,臭氧气流量0.06 m3 h 1,混合溶剂中水的质量含量为15%,反应时间100 min,茴香醛产率82.70%。该反应在水的存在下实现了室温下一步法合成茴香醛,避免了茴脑臭氧化物的分离及还原步骤,工艺简单,洁净环保。

At room temperature, the anisaldehyde of anethole （1-methoxy-4-（1 -propenyl）-benzene） （4-methoxybenzaldehyde） was synthesized by the ozonolysis in a novel and environmentally friendly mixture solvent system which was composed of organic solvent and water, The product was characterized by GC-MS, FT-IR and 1H-NMR spectra. The yields of anisaldehyde from organic solvent / water systems were compared with those from traditional solvent systems. The acetone / water solvent was chosen to be the optimal solvent system. Meanwhile, the effects of the solvent species, solvent quantity, 03 / 02 flow, water content in the mixture solvent and the reaction time on the reaction were investigated. By FT-IR and UV spectra, the reaction mechanism was investigated. It was found that, when 03 / Oz flow is 0.06 m3.h-1, the highest yield up to 82.70% can be obtained under the condition of using water / acetone as solvent system （water ratio in this solvent is 15%, m （anethole） / m （solvent） is 1 / 3）, reaction time of 100 minutes and at room temperature. Compared with the traditional ozonolysis process, with the presence of water, ozonolysis of anethole results in the direct formation of anisaldehyde at room temperature and avoids the isolation or decomposition of ozonide. It is a convenient and environment friendly technology.